CN114136874A - Device and method for measuring metal corrosion resistance under high temperature and high pressure - Google Patents
Device and method for measuring metal corrosion resistance under high temperature and high pressure Download PDFInfo
- Publication number
- CN114136874A CN114136874A CN202111424871.2A CN202111424871A CN114136874A CN 114136874 A CN114136874 A CN 114136874A CN 202111424871 A CN202111424871 A CN 202111424871A CN 114136874 A CN114136874 A CN 114136874A
- Authority
- CN
- China
- Prior art keywords
- corrosion
- metal
- quartz capillary
- test piece
- capillary tube
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/006—Investigating resistance of materials to the weather, to corrosion, or to light of metals
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Biodiversity & Conservation Biology (AREA)
- Ecology (AREA)
- Environmental & Geological Engineering (AREA)
- Environmental Sciences (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
Abstract
The invention discloses a device and a method for measuring the corrosion resistance of metal under high temperature and high pressure, wherein the method comprises the following steps: heating a quartz capillary tube filled with corrosive liquid and a metal test piece to a set temperature, and performing in-situ detection by using Raman spectroscopy every 0.5-2 days to deduce the corrosion degree of the metal test piece; if no corrosion occurs or the corrosion degree is small, continuing to perform the simulated corrosion experiment; if the metal test piece is inferred to be obviously corroded through the Raman spectrum in-situ detection, the simulated corrosion experiment is recorded to be finished, the total corrosion time of the heat preservation experiment at the set temperature is recorded, the quartz capillary tube is unsealed, and the metal test piece and the corrosive liquid are taken out to be respectively subjected to corrosion data test and acquisition. The method can be used for measuring the corrosion resistance of metal at high temperature and high pressure, and the quartz capillary tube device is transparent and visible, can be used for in-situ detection, has low manufacturing cost and convenient operation, and simultaneously solves a series of problems that metal components of a reaction kettle are easy to interfere with corrosion and the like in the prior art.
Description
Technical Field
The invention belongs to the technical field of chemical industry, materials and environment, and particularly relates to a device and a method for measuring the corrosion resistance of metal at high temperature and high pressure.
Background
In industrial production, wastewater treatment and other processes, metal materials are widely used due to their excellent properties, but the corrosion problem is also highlighted. At present, the research on the corrosion resistance of metal in normal-temperature and normal-pressure corrosive liquid is mature, but the research on the corrosion in high-temperature and high-pressure corrosive liquid is relatively insufficient. Therefore, the development of a device and a method for measuring the corrosion resistance of the metal under high temperature and high pressure has great significance in the fields of chemical industry, materials, environment and the like.
However, in the conventional technology, the high-temperature and high-pressure corrosion research usually adopts a high-temperature and high-pressure reaction kettle made of metal to achieve the high-temperature and high-pressure conditions, and the device usually uses a pressure reducing valve or a pressure pump to control the pressure, so that the operation is complicated and the device is complex; moreover, the device can not be visualized generally, and the corrosion condition can not be detected in situ; also, since the device is made of a metallic material, the metallic elements thereof interfere with the corrosion results.
Therefore, in order to accurately obtain data on metal corrosion in high-temperature and high-pressure corrosive liquid, an apparatus and a method capable of avoiding the above problems are needed.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention aims to provide a device and a method for measuring the corrosion resistance of metal at high temperature and high pressure.
The method for measuring the corrosion resistance of the metal at high temperature and high pressure is characterized by comprising the following steps of:
1) filling a quartz capillary tube which is filled with corrosive liquid and a metal test piece inside and has two sealed ends into a copper heating sleeve;
2) placing the copper heating sleeve in a tubular heating furnace, heating to a set temperature, and then preserving heat to enable the corrosive liquid in the quartz capillary tube to enter a high-temperature and high-pressure state at the set temperature, and carrying out a simulated corrosion experiment;
3) step 2) in the simulated corrosion experiment, carrying out qualitative test operation on the metal corrosion degree every 0.5-2 days, namely stopping heating the tubular heating furnace and cooling to room temperature, then taking out the quartz capillary tube, carrying out in-situ detection by using Raman spectrum, and analyzing the form changes of the corrosion liquid and the metal test piece in the quartz capillary tube so as to deduce the corrosion degree of the metal test piece;
4) step 3) when the metal corrosion degree is qualitatively tested, if the Raman spectrum in-situ detection analysis concludes that the metal test piece is not corroded or the corrosion degree is small, the quartz capillary tube is refilled into the copper heating sleeve, and the temperature is raised to the set temperature by using the tubular heating furnace to carry out a simulated corrosion experiment; if the metal test piece is judged to be obviously corroded, the corrosion test is recorded as the end of a simulated corrosion test, the total corrosion time of the heat preservation test at the set temperature is recorded, the quartz capillary tube is unsealed, and the metal test piece and the corrosive liquid are taken out to be respectively subjected to corrosion data test acquisition.
The method for measuring the corrosion resistance of the metal at high temperature and high pressure is characterized in that the corrosive liquid comprises wastewater and hydrogen peroxide with the mass concentration of 10-40%, oxygen is an oxidant commonly used for supercritical water oxidation, and hydrogen peroxide is a source for providing oxygen. The wastewater is wastewater from an enterprise or simulated wastewater prepared by an experiment.
The method for measuring the corrosion resistance of the metal under high temperature and high pressure is characterized in that other simulated gas is also filled in the quartz capillary tube, and the other simulated gas is CO2、CO、O2Etc. to simulate a corrosive environment under different gas conditions.
The method for measuring the metal corrosion resistance under high temperature and high pressure is characterized in that the manufacturing method of the quartz capillary comprises the following steps:
s1: cutting a certain length of quartz capillary, and welding and sealing one end of the quartz capillary by using hydrogen flame;
s2: adding a metal test piece into the sealed end of the quartz capillary, and injecting corrosive liquid through the miniature sample injection needle, wherein the corrosive liquid forms a liquid seal at one end of the metal test piece facing the open end of the quartz capillary;
s3: after the operation of the step S2 is finished, if a corrosion environment including other gases needs to be simulated, the quartz capillary tube is placed in a liquid nitrogen environment, other gases are continuously introduced into the quartz capillary tube, the corrosion liquid and the gases are frozen to be solid by using the liquid nitrogen, and then the next operation is carried out; if not, directly entering the next operation;
s4: and welding and sealing the other end of the quartz capillary tube by using hydrogen flame to obtain the quartz tube reactor filled with the metal test piece, the corrosive liquid and the gas.
The method for measuring the metal corrosion resistance under high temperature and high pressure is characterized in that the inner diameter of the quartz capillary tube is 1.9-2.1mm, the outer diameter is less than 4mm, and the outer diameter of the metal test piece is less than the inner diameter of the quartz capillary tube; the length of the quartz capillary tube is smaller than the filling length of the copper heating sleeve.
The method for measuring the corrosion resistance of the metal at high temperature and high pressure is characterized in that in the step 4), the method for carrying out corrosion data test acquisition comprises at least one of the following steps:
m1: after the corrosion is finished, the quartz capillary tube is unsealed, the metal test piece is cleaned by clear water, dried and weighed, the weight is compared with the weight before the corrosion, and the corrosion rate of the metal is calculated;
m2: observing the physical appearance of the surface and the cross section of the metal test piece by using a scanning electron microscope, comparing with the physical appearance before corrosion, and further qualitatively inferring the metal corrosion degree;
m3: detecting surface elements of the metal test piece by using an energy spectrometer, combining physical appearances of the surface and the cross section of the metal test piece observed by a scanning electron microscope, analyzing the thickness and components of an oxide film on the surface of the metal test piece, comparing the thickness and the components with those before corrosion, and estimating the corrosion rate of the metal test piece according to the oxygen content of the surface of the metal test piece and the change of the thickness of the oxide film;
m4: analyzing the surface of the metal test piece by using an X-ray diffractometer, comparing with the surface before corrosion, and analyzing a corrosion product;
m5: and detecting the composition and content of metal ions in the corrosion liquid, comparing with the composition and content before corrosion, and calculating the corrosion rate according to the concentration of the metal ions. For example, the ion composition in the etching solution can be analyzed by techniques such as X-ray fluorescence spectroscopy, atomic absorption spectrophotometer, plasma emission spectroscopy, or ion chromatography.
The device used in the method for measuring the corrosion resistance of the metal at high temperature and high pressure is characterized by comprising a quartz capillary tube, a copper heating sleeve and a tubular heating furnace; the quartz capillary tube is filled with a metal test piece and corrosive liquid, the quartz capillary tube is filled in a copper heating sleeve, and the copper heating sleeve is placed in a tubular heating furnace for temperature regulation and control.
Further, copper heating tube is the cylinder structure, and copper heating tube is last evenly to be provided with the ascending pipe chamber of placing of a plurality of openings at interval, and the degree of depth of placing the pipe chamber is greater than quartz capillary's length, and quartz capillary's external diameter is less than the internal diameter of placing the pipe chamber a little, and quartz capillary cooperation is placed in placing the pipe chamber on copper heating tube.
Furthermore, the tubular heating furnace comprises a furnace body, wherein a sleeve placing cavity with an upward opening is formed in the furnace body, and a copper heating sleeve can be placed in the sleeve placing cavity of the furnace body in a matched manner; the furnace body is also provided with a furnace cover, and the upper end opening of the sleeve containing cavity can be closed when the furnace cover is closed.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention takes the quartz capillary as the reactor, has low manufacturing cost and simple and easy manufacture, can manufacture a plurality of quartz capillaries to simultaneously carry out experiments of a plurality of groups of different reaction conditions (such as metal types, corrosive media, oxidants and the like), has high experimental efficiency, and can not reach the efficiency of the quartz tube reactor when purchasing a common high-temperature high-pressure reaction kettle with the same cost.
2. The quartz capillary tube selected by the invention has small volume and visible whole body, can be moved to a characterization instrument for in-situ detection (such as metal oxide layer analysis by using Raman) in the middle stage of an experiment so as to keep the original experiment condition unchanged, and the common high-temperature high-pressure reaction kettle has large volume, is difficult to be used together with the characterization instrument, generally needs to take out metal for characterization, so that the experiment condition is changed and the experiment result is interfered.
3. According to the invention, the quartz capillary is used as the reactor, so that no external metal is contacted with the corrosive liquid, interference detection caused by other metal ions entering the corrosive liquid is avoided, and metal ions can possibly enter the corrosive liquid in the metal lining of a common reaction kettle under the conditions of high temperature and high pressure.
4. The invention takes the volume expansion generated after the corrosive liquid enters a high-temperature and high-pressure state as a pressure generation source, controls the pressure in the corrosion process through the adding amount of the corrosive liquid, has simple and convenient operation and simple device, and improves the efficiency, while the pressure of a common high-temperature and high-pressure reaction kettle is usually regulated and controlled through a pressure reducing valve and a pressure pump, and the device is complicated and has complex operation.
5. According to the invention, the quartz capillary tube is used as the reaction kettle, the metal to be detected cannot be damaged in the corrosion simulation process, the corrosion environment conforms to the actual working condition, the metal to be detected and the corrosive liquid are less, the experiment cost is saved, and the selection of the metal material in the industrial environment is favorably guided.
Drawings
FIG. 1 is a schematic structural diagram of a quartz capillary tube made in accordance with the present invention;
FIG. 2 is a schematic structural view of a copper heating sleeve according to the present invention;
FIG. 3 is a schematic view of the structure of the tube furnace of the present invention;
in the figure: 1-quartz tube reactor, 2-copper heating sleeve, 3-tube heating furnace, 4-metal test piece and 5-corrosive liquid.
Detailed Description
The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention.
Example (b): compare FIGS. 1-3
The invention relates to a device for measuring the metal corrosion resistance under high temperature and high pressure, which comprises a quartz capillary 1, a copper heating sleeve 2 and a tubular heating furnace 3. A metal test piece 4 and a corrosive liquid 5 are filled in a quartz capillary tube 1, the quartz capillary tube 1 is filled in a copper heating sleeve 2, and the copper heating sleeve 2 is placed in a tubular heating furnace 3 for temperature regulation.
The tubular heating furnace 3 comprises a furnace body, a sleeve placing cavity with an upward opening is formed in the furnace body, and the copper heating sleeve 2 can be placed in the sleeve placing cavity of the furnace body in a matched mode; the furnace body is also provided with a furnace cover, and the upper end opening of the sleeve containing cavity can be closed when the furnace cover is closed.
In the invention, the inner diameter of the quartz capillary tube is 1.9-2.1mm, the outer diameter is less than 4mm, and the outer diameter of the metal test piece is less than the inner diameter of the quartz capillary tube; the length of the quartz capillary tube is smaller than the filling length of the copper heating sleeve (namely the depth of the placing cavity of the copper heating sleeve).
The manufacturing method of the quartz capillary tube comprises the following steps:
s1: cutting a certain length of quartz capillary, and welding and sealing one end of the quartz capillary by using hydrogen flame;
s2: adding a metal test piece into the sealed end of the quartz capillary, and injecting corrosive liquid through the miniature sample injection needle, wherein the corrosive liquid forms a liquid seal at one end of the metal test piece facing the open end of the quartz capillary;
s3: after the operation of the step S2 is finished, if a corrosion environment including other gases needs to be simulated, the quartz capillary tube is placed in a liquid nitrogen environment, other gases are continuously introduced into the quartz capillary tube, the corrosion liquid and the gases are frozen to be solid by using the liquid nitrogen, and then the next operation is carried out; if not, directly entering the next operation;
s4: and welding and sealing the other end of the quartz capillary tube by using hydrogen flame to obtain the quartz tube reactor filled with the metal test piece, the corrosive liquid and the gas.
Example 1:
a series of 60mm long, 2mm internal diameter quartz tubes were cut, and a series of 20mm long, 1.7mm diameter metal test specimens (Zr, TA9 or TA10) were cut and weighed separately.
When the quartz capillary tube is manufactured, firstly, one end of the quartz tube is sealed by oxyhydrogen flame, then the weighed metal sample to be measured is placed into the quartz capillary tube, then, a miniature sample injection needle is used for injecting corrosive liquid into the quartz tube, and the other end of the quartz capillary tube is sealed by oxyhydrogen flame welding, so that the miniature high-temperature high-pressure balance kettle filled with the metal sample to be measured and the corrosive liquid is obtained. Wherein, 25uL perchloric acid wastewater and 5uL 30 wt% hydrogen peroxide are used as corrosive liquid. The perchloric acid waste water is prepared by taking organic chlorine waste water with salinity of 24.5% and COD of 12000 from a factory and adjusting the pH value to 2.5 by hydrochloric acid.
And respectively putting a plurality of welded and sealed quartz capillary tubes into copper heating sleeves. And placing the copper heating sleeve in a tubular heating furnace, heating the copper heating sleeve to 380 ℃ from room temperature within 30min, regulating and stabilizing the copper heating sleeve at 380 ℃, heating the copper heating sleeve to 380 ℃, and then preserving heat to enable the corrosive liquid in the quartz capillary to enter a high-temperature high-pressure state (25MPa) at a set temperature to perform a simulated corrosion experiment. In the corrosion process, the Raman spectrum in-situ detection quartz tube reactor is used every day to analyze the component changes of the corrosion liquid, the surface of the metal test piece and the gas and deduce the corrosion degree. Through Raman spectrum in-situ qualitative analysis, results of comparison of results of 100 hours, 360 hours and 720 hours before corrosion and after corrosion show that the corrosion resistance of TA9 and TA10 in perchloric acid wastewater is superior to that of Zr, and the corrosion resistance of TA9 is superior to that of TA 10.
After the total corrosion time is 100 hours, 360 hours and 720 hours, the part of the quartz tube reactor is unsealed, the metal test piece and the corrosion liquid are taken out, the metal test piece is firstly cleaned by clean water, then dried and weighed, and compared with the weight before corrosion, the corrosion rate of the metal is calculated. And then detecting the surface elements of the metal test piece by using an energy spectrometer, combining the physical appearances of the surface and the cross section of the metal test piece observed by a scanning electron microscope, analyzing the thickness and the components of the oxide film on the surface of the metal test piece, comparing the thickness and the components with those before corrosion, and estimating the corrosion rate of the metal test piece according to the oxygen content of the surface of the metal test piece and the change of the thickness of the oxide film. The corrosion products were analyzed using an X-ray diffractometer. And then analyzing the composition and content of metal ions in the corrosive liquid by an X-ray fluorescence spectrum, an atomic absorption spectrophotometer, a plasma emission spectrum or an ion chromatography, comparing with the composition and content before corrosion, and calculating the corrosion rate according to the concentration of the metal ions.
Wherein the calculation of the corrosion rate was performed by weighing method for Zr, TA9 and TA10, respectively, before the corrosion experiment, and after the corrosion was performed for a total of 720 hours. After the corrosion is finished, the quartz capillary tube is unsealed, the metal test piece is cleaned by clear water and then dried, weighed, compared with the weight before the corrosion, and the corrosion rate of the metal is calculated by the following calculation formula:
x-test piece corrosion rate mm/a
W1-weighing g of test pieces before testing
W2-test piece weighing g after test
87600-calculating constants
A-test piece surface area cm2
T-test time h
D-density of specimen material g/cm3
According to the experimental process, the corrosion rate of Zr in the acidic high-chlorine wastewater is 0.18mm/A, TA9 is 0.08mm/A and TA10 is 0.11mm/A before and after the corrosion lasts for 720 hours, which is basically consistent with the observation result of Raman spectrum in-situ qualitative analysis.
The statements in this specification merely set forth a list of implementations of the inventive concept and the scope of the present invention should not be construed as limited to the particular forms set forth in the examples.
Claims (9)
1. A method for measuring the corrosion resistance of metal under high temperature and high pressure is characterized by comprising the following steps:
1) filling a quartz capillary tube which is filled with corrosive liquid and a metal test piece inside and has two sealed ends into a copper heating sleeve;
2) placing the copper heating sleeve in a tubular heating furnace, heating to a set temperature, and then preserving heat to enable the corrosive liquid in the quartz capillary tube to enter a high-temperature and high-pressure state at the set temperature, and carrying out a simulated corrosion experiment;
3) step 2) in the simulated corrosion experiment, carrying out qualitative test operation on the metal corrosion degree every 0.5-2 days, namely stopping heating the tubular heating furnace and cooling to room temperature, then taking out the quartz capillary tube, carrying out in-situ detection by using Raman spectrum, and analyzing the form changes of the corrosion liquid and the metal test piece in the quartz capillary tube so as to deduce the corrosion degree of the metal test piece;
4) step 3) when the metal corrosion degree is qualitatively tested, if the Raman spectrum in-situ detection analysis concludes that the metal test piece is not corroded or the corrosion degree is small, the quartz capillary tube is refilled into the copper heating sleeve, and the temperature is raised to the set temperature by using the tubular heating furnace to carry out a simulated corrosion experiment; if the metal test piece is judged to be obviously corroded, the corrosion test is recorded as the end of a simulated corrosion test, the total corrosion time of the heat preservation test at the set temperature is recorded, the quartz capillary tube is unsealed, and the metal test piece and the corrosive liquid are taken out to be respectively subjected to corrosion data test acquisition.
2. The method according to claim 1, wherein the corrosion-resistant liquid comprises waste water, and the waste water is waste water from an enterprise or experimentally prepared simulated waste water.
3. The method for measuring the metal corrosion resistance at high temperature and high pressure as claimed in claim 2, wherein the corrosive liquid comprises wastewater and hydrogen peroxide with the mass concentration of 10-40%; other simulation gases are also filled in the quartz capillary tube, and the other simulation gases are CO2、CO、O2At least one of (1).
4. The method for measuring the corrosion resistance of a metal at high temperature and high pressure according to claim 1, wherein the quartz capillary is fabricated by a method comprising the steps of:
s1: cutting a certain length of quartz capillary, and welding and sealing one end of the quartz capillary by using hydrogen flame;
s2: adding a metal test piece into the sealed end of the quartz capillary, and injecting corrosive liquid through the miniature sample injection needle, wherein the corrosive liquid forms a liquid seal at one end of the metal test piece facing the open end of the quartz capillary;
s3: after the operation of the step S2 is finished, if a corrosion environment including other gases needs to be simulated, the quartz capillary tube is placed in a liquid nitrogen environment, other gases are continuously introduced into the quartz capillary tube, the corrosion liquid and the gases are frozen to be solid by using the liquid nitrogen, and then the next operation is carried out; if not, directly entering the next operation;
s4: and welding and sealing the other end of the quartz capillary tube by using hydrogen flame to obtain the quartz tube reactor filled with the metal test piece, the corrosive liquid and the gas.
5. The method for measuring the corrosion resistance of metal under high temperature and high pressure as claimed in claim 1, wherein the quartz capillary has an inner diameter of 1.9-2.1mm and an outer diameter of 4mm or less, and the outer diameter of the metal specimen is smaller than the inner diameter of the quartz capillary; the length of the quartz capillary tube is smaller than the filling length of the copper heating sleeve.
6. The method for determining the corrosion resistance of metal at high temperature and high pressure according to claim 1, wherein in the step 4), the method for performing the corrosion data test acquisition comprises at least one of the following:
m1: after the corrosion is finished, the quartz capillary tube is unsealed, the metal test piece is cleaned by clear water, dried and weighed, the weight is compared with the weight before the corrosion, and the corrosion rate of the metal is calculated;
m2: observing the physical appearance of the surface and the cross section of the metal test piece by using a scanning electron microscope, comparing with the physical appearance before corrosion, and further qualitatively inferring the metal corrosion degree;
m3: detecting surface elements of the metal test piece by using an energy spectrometer, combining physical appearances of the surface and the cross section of the metal test piece observed by a scanning electron microscope, analyzing the thickness and components of an oxide film on the surface of the metal test piece, comparing the thickness and the components with those before corrosion, and estimating the corrosion rate of the metal test piece according to the oxygen content of the surface of the metal test piece and the change of the thickness of the oxide film;
m4: analyzing the surface of the metal test piece by using an X-ray diffractometer, comparing with the surface before corrosion, and analyzing a corrosion product;
m5: and detecting the composition and content of metal ions in the corrosion liquid, comparing with the composition and content before corrosion, and calculating the corrosion rate according to the concentration of the metal ions.
7. The apparatus for measuring the corrosion resistance of metal under high pressure and high temperature according to claim 1, which comprises a quartz capillary (1), a copper heating sleeve (2) and a tube furnace (3); the device comprises a quartz capillary tube (1), a metal test piece (4) and corrosive liquid (5) are arranged in the quartz capillary tube (1), the quartz capillary tube (1) is arranged in a copper heating sleeve (2), and the copper heating sleeve (2) is arranged in a tubular heating furnace (3) for temperature regulation.
8. The device according to claim 7, characterized in that the copper heating sleeve (2) is a cylinder structure, a plurality of placing tube cavities with upward openings are uniformly arranged on the copper heating sleeve (2) at intervals, the depth of the placing tube cavities is larger than the length of the quartz capillary tube (1), the outer diameter of the quartz capillary tube (1) is slightly smaller than the inner diameter of the placing tube cavities, and the quartz capillary tube (1) is fittingly placed in the placing tube cavities on the copper heating sleeve (2).
9. The device according to claim 7, characterized in that the tubular heating furnace (3) comprises a furnace body, a sleeve placing cavity with an upward opening is arranged on the furnace body, and the copper heating sleeve (2) can be placed in the sleeve placing cavity of the furnace body in a matching way; the furnace body is also provided with a furnace cover, and the upper end opening of the sleeve containing cavity can be closed when the furnace cover is closed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111424871.2A CN114136874B (en) | 2021-11-26 | 2021-11-26 | Device and method for measuring corrosion resistance of metal at high temperature and high pressure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111424871.2A CN114136874B (en) | 2021-11-26 | 2021-11-26 | Device and method for measuring corrosion resistance of metal at high temperature and high pressure |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114136874A true CN114136874A (en) | 2022-03-04 |
| CN114136874B CN114136874B (en) | 2023-08-08 |
Family
ID=80388681
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111424871.2A Active CN114136874B (en) | 2021-11-26 | 2021-11-26 | Device and method for measuring corrosion resistance of metal at high temperature and high pressure |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114136874B (en) |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2635805A1 (en) * | 2008-06-12 | 2009-12-12 | Northern Alberta Institute Of Technology | Gas chromatography capillary devices and methods |
| CN102539272A (en) * | 2011-12-21 | 2012-07-04 | 西安交通大学 | Experimental device and representation method of multiphase medium high-temperature corrosion rate |
| CN104931372A (en) * | 2015-06-03 | 2015-09-23 | 中国石油大学(华东) | Experimental method for simulating stress corrosion of metal material under working conditions |
| CN105223127A (en) * | 2014-07-02 | 2016-01-06 | 西南石油大学 | A kind of visual reaction experiment device of high temperature resistant, high pressure |
| US20170016856A1 (en) * | 2014-12-31 | 2017-01-19 | Nuctech Company Limited | Detection apparatus and detection method |
| CN108426868A (en) * | 2018-03-13 | 2018-08-21 | 浙江工业大学 | The method of on-line determination carbon dioxide solubility in pure water in situ |
| CN210646283U (en) * | 2019-08-08 | 2020-06-02 | 金光宇 | Visual miniature high-temperature high-pressure quartz capillary balance kettle capable of measuring pressure |
| CN111693508A (en) * | 2020-06-16 | 2020-09-22 | 浙江工业大学 | Quartz reaction kettle device for in-situ online monitoring of low-temperature high-pressure reaction |
| CN113029857A (en) * | 2021-03-05 | 2021-06-25 | 浙江工业大学 | Device and method for measuring solubility of hydrophobic organic matters in water |
-
2021
- 2021-11-26 CN CN202111424871.2A patent/CN114136874B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2635805A1 (en) * | 2008-06-12 | 2009-12-12 | Northern Alberta Institute Of Technology | Gas chromatography capillary devices and methods |
| CN102539272A (en) * | 2011-12-21 | 2012-07-04 | 西安交通大学 | Experimental device and representation method of multiphase medium high-temperature corrosion rate |
| CN105223127A (en) * | 2014-07-02 | 2016-01-06 | 西南石油大学 | A kind of visual reaction experiment device of high temperature resistant, high pressure |
| US20170016856A1 (en) * | 2014-12-31 | 2017-01-19 | Nuctech Company Limited | Detection apparatus and detection method |
| CN104931372A (en) * | 2015-06-03 | 2015-09-23 | 中国石油大学(华东) | Experimental method for simulating stress corrosion of metal material under working conditions |
| CN108426868A (en) * | 2018-03-13 | 2018-08-21 | 浙江工业大学 | The method of on-line determination carbon dioxide solubility in pure water in situ |
| CN210646283U (en) * | 2019-08-08 | 2020-06-02 | 金光宇 | Visual miniature high-temperature high-pressure quartz capillary balance kettle capable of measuring pressure |
| CN111693508A (en) * | 2020-06-16 | 2020-09-22 | 浙江工业大学 | Quartz reaction kettle device for in-situ online monitoring of low-temperature high-pressure reaction |
| CN113029857A (en) * | 2021-03-05 | 2021-06-25 | 浙江工业大学 | Device and method for measuring solubility of hydrophobic organic matters in water |
Non-Patent Citations (2)
| Title |
|---|
| KE BEI 等: "Solubility and dissolution mechanism of 4-chlorotoluene in subcritical water investigated in a fused silica capillary reactor by in situ Raman spectroscopy", 《FLUID PHASE EQUILIBRIA》, pages 93 - 97 * |
| 林春绵 等: "氯苯类污染物超临界水氧化反应动力学研究", 发酵科技通讯, vol. 47, no. 2, pages 65 - 70 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114136874B (en) | 2023-08-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP3531736B2 (en) | Carburizing method and carburizing device | |
| CN101718725B (en) | Device for measuring sample thermo-physical property in situ | |
| CN106501125B (en) | Gas adsorption and desorption testing device and testing method | |
| US8754369B2 (en) | System and method for measuring hydrogen content in a sample | |
| Pauss et al. | Continuous measurement of dissolved H2 in an anaerobic reactor using a new hydrogen/air fuel cell detector | |
| CN106092691B (en) | Solid hydrogen-containing sample hydrogen isotope on-line sample preparation facilities | |
| CN114136874A (en) | Device and method for measuring metal corrosion resistance under high temperature and high pressure | |
| RU2341790C1 (en) | Method of gas sensor calibration | |
| Baichi et al. | Thermodynamics of the O–U system. IV–Critical assessment of chemical potentials in the U–UO2. 01 composition range | |
| CN111638263A (en) | Gas sampling and analyzing device and method | |
| CN108303297B (en) | Dual-purpose hydrogen method and zinc method 14 C sample preparation system | |
| CN113252529B (en) | High-temperature gas-driven penetration testing system and method for metal pipe fitting | |
| Boyd et al. | Determination of the abundance and isotope composition of nitrogen within organic compounds: a sealed tube technique for use with static vacuum mass spectrometers | |
| CN111239038A (en) | Simulation device for on-line continuous monitoring of metal local corrosion process and determination method thereof | |
| Wang et al. | A new CF-IRMS system for quantifying stable isotopes of carbon monoxide from ice cores and small air samples | |
| Satar et al. | Towards an understanding of surface effects: testing of various materials in a small volume measurement chamber and its relevance for atmospheric trace gas analysis | |
| RU36889U1 (en) | LIQUID SAMPLE PREPARATION DEVICE FOR ISOTOPIC ANALYSIS OF HYDROGEN | |
| KR101193988B1 (en) | Apparatus for analyzing gas phase response in multiplex environment | |
| CN112986327B (en) | Rapid heating-atmosphere variable-weight real-time thermal analysis device and application | |
| US20220307959A1 (en) | A Device For Determining A Volume Of Gas In A Sample | |
| Alex | Development of New Methods to Control Redox Conditions in High-Pressure Experiments and Their Application to Study Ore Metal Solubilities in Sulfur-Bearing Magmatic Fluids | |
| JP6696393B2 (en) | Method for producing test solution used for stress corrosion cracking test of stainless steel, and stress corrosion cracking test method for stainless steel | |
| Hofmann | The High-pO2 Method to Prevent U-Loss During Single-Aliquot Hematite (U-Th)/He Measurement: Development, Implementation, and Automation | |
| JP3328448B2 (en) | Metal sample decomposition device | |
| CN111398348A (en) | Natural gas amine decarburization reaction heat measurement system based on adiabatic calorimetry and reaction heat measurement method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |